CN109219577B - Preparation of nanoparticulate titanium dioxide - Google Patents

Preparation of nanoparticulate titanium dioxide Download PDF

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CN109219577B
CN109219577B CN201780033832.5A CN201780033832A CN109219577B CN 109219577 B CN109219577 B CN 109219577B CN 201780033832 A CN201780033832 A CN 201780033832A CN 109219577 B CN109219577 B CN 109219577B
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titanium dioxide
nanoparticulate
alkali
neutralization
filter cake
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CN109219577A (en
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海因茨-克里斯蒂安·克伦普尔
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Kronos International Inc
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    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28004—Sorbent size or size distribution, e.g. particle size
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/2803—Sorbents comprising a binder, e.g. for forming aggregated, agglomerated or granulated products
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/063—Titanium; Oxides or hydroxides thereof
    • B01J35/23—
    • B01J35/39—
    • B01J35/40—
    • B01J35/615—
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B01J37/0027—Powdering
    • B01J37/0036—Grinding
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
    • C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
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    • B01D2253/112—Metals or metal compounds not provided for in B01D2253/104 or B01D2253/106
    • B01D2253/1124—Metal oxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D2255/00—Catalysts
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    • B01D2255/20707—Titanium
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
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    • B01D2255/802—Photocatalytic
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    • B01D—SEPARATION
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    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
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    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds

Abstract

The present invention relates to a process for obtaining nanoparticulate titanium dioxide in agglomerated form from hydrolysed acidic titanium oxides, the titanium dioxide thus obtained and its use as photocatalyst, process catalyst or adsorbent, in particular in aqueous systems.

Description

Preparation of nanoparticulate titanium dioxide
Technical Field
The present invention relates to a process for obtaining nanoparticulate titanium dioxide in agglomerated form from hydrolysed acidic titanium oxides, the titanium dioxide thus obtained and its use as photocatalyst, process catalyst or adsorbent, in particular in aqueous systems.
Background
Nanoparticulate titanium dioxide is widely used as an adsorbent, a process catalyst or a photocatalyst due to its high specific surface area and semiconductor characteristics. Commercial production of nanoparticulate titania is typically achieved by hydrolysis of acidic titanyl compounds (e.g., titanyl chloride or sulfate) followed by heat treatment. For example, titanyl sulfate is produced by sulfuric acid digestion of a titaniferous material, such as ilmenite.
In the case of using titanyl sulfate as a starting compound, the titanium oxide-hydrate (metatitanic acid) formed by hydrolysis of titanyl sulfate is separated from the acidic suspension and washed to remove other metal salts and attached sulfuric acid. Furthermore, the titanium oxide hydrate must be neutralized, since in general 5 to 10% by weight of chemisorbed sulfuric acid remains despite intensive washing. This neutralization is generally carried out by means of basic compounds, such as sodium hydroxide or calcium hydroxide, as disclosed in DE 10392330B4 and CN 104209108A.
The use of calcium hydroxide (also known as milk of lime) in the neutralization step results in the formation of slightly soluble calcium sulfate, resulting in porous agglomerates of titanium dioxide and calcium sulfate as product. However, neutralization with calcium hydroxide can lead to filter cake breakage during washing, making it impossible to wash the filter cake vigorously. In addition, the calcium sulfate formed exhibits residual solubility of calcium ions in aqueous systems.
Despite the formation of readily soluble sodium sulfate (which can be washed off completely) during neutralization with sodium hydroxide, a very finely divided titanium dioxide product is obtained which is difficult to handle.
Thus, there is a need for a process for the neutralization of acidic titanium oxide-hydrates that produces a nanoparticle agglomerated titanium dioxide product in which an easily washable filter cake and insoluble compounds are formed.
Disclosure of Invention
It is an object of the present invention to provide a neutralization process for titanium oxide-hydrates which contain sulfuric acid and are to be further processed into nanoparticulate titanium dioxide product, in which process insoluble compounds and a readily washable filter cake are formed.
The inventors have surprisingly found that a process for preparing nanoparticulate titanium dioxide comprises the following steps: (i) providing an aqueous solution of an acidic titanyl compound; (ii) hydrolyzing the titanyl compound to produce a titanium oxide-hydrate suspension; (iii) filtering the suspension and washing the resulting titanium oxide-hydrate filter cake; (iv) neutralizing the filter cake; (v) heat treatment of the filter cake, characterized in that said neutralization is effected by adding an aqueous solution of an alkali silicate and/or alkali aluminate to obtain a nanoparticulate titanium dioxide product, wherein insoluble compounds and a readily washable filter cake are formed.
Accordingly, in a first aspect, the present invention relates to a process for preparing nanoparticulate titania comprising the steps of:
(i) providing an aqueous solution of an acidic titanyl compound;
(ii) hydrolyzing the titanyl compound to produce a titanium oxide-hydrate suspension;
(iii) filtering the suspension and washing the resulting titanium oxide-hydrate filter cake;
(iv) neutralizing the filter cake; and
(v) heat treating the filter cake;
characterized in that the neutralization is effected by adding an aqueous solution of an alkali silicate and/or an alkali aluminate.
In another aspect, the present invention relates to titanium dioxide obtainable by the process described herein.
Finally, in a further aspect, the present invention relates to the use of the nanoparticulate titanium obtainable by the process described herein as an adsorbent, a photocatalyst or a process catalyst.
Further advantageous embodiments of the invention are described in the dependent claims.
Detailed Description
These and other aspects, features and advantages of the present invention will become apparent to those skilled in the art upon review of the following detailed description and claims. Each feature from one aspect of the invention may also be used in any other aspect of the invention. The numerical ranges stated in the form "from x to y" include the numerical values mentioned and the numerical values within the corresponding measurement accuracy ranges known to the person skilled in the art. If several preferred numerical ranges are set forth in this form, all ranges formed by combinations of the various endpoints are also encompassed. All percentages relating to the compositions described herein refer to weight percentages, based on the mixture of the compositions, respectively, unless explicitly stated otherwise.
Within the scope of the present invention, "nanoparticulate titanium dioxide" means titanium dioxide having a primary particle diameter of up to 100 nm. As used herein, a "primary particle" is a particle that can be formed with at least one other particle in agglomerates and aggregates. Such definition of primary particles also covers pairs of particles and pluralities of pairs of particles, which are known in the art and can be analyzed by e.g. TEM analysis.
The present invention begins with an aqueous solution of an acidic titanyl compound. For example, titanyl sulfate or titanium oxychloride is suitable as the titanyl compound. Titanyl sulfate is particularly preferred.
A particular embodiment of the invention starts with a titanyl sulfate solution prepared by sulfuric acid digestion of a titaniferous feed material, such as ilmenite. Such titanyl sulfate solutions are obtained, for example, during the known process for preparing titanium dioxide pigments according to the sulfate process. In the titanyl sulfate solution, water-soluble salts (e.g., iron sulfate) are crystallized out and separated. Subsequently, the titanyl compound is hydrolyzed, and a titanium oxide hydrate is precipitated. The precipitated microcrystalline titanium oxide-hydrate is separated by filtration, washed and the filter cake neutralized.
According to the invention, the filter cake is neutralized with an alkali silicate solution (water glass) and/or an alkali aluminate solution. The alkali silicate solution preferably contains sodium silicate and/or potassium silicate and/or lithium silicate at a concentration of 2-20 mole percent. The alkali aluminate solution preferably contains sodium aluminate in a concentration of 2 to 20 mole percent. Within the scope of the present invention, "neutralization" means that the pH is adjusted to a value in the range of 4 to 9. More preferably, an alkali aluminate solution is used.
The neutralization is carried out, for example, in a vessel in which the washed filter cake (optionally diluted with water) is mixed with the alkali silicate or sodium aluminate solution with stirring. In the case of titanyl sulfate from the sulfate process for the production of titanium dioxide, the filter cake of washed titanium oxide-hydrate hydrolysate typically has a pH of 1 to 2 prior to neutralization.
Upon neutralization with an alkali silicate, a readily soluble and washable alkali sulfate (including but not limited to sodium, potassium and/or lithium sulfate) and insoluble silica are formed as reaction products. During neutralization with sodium aluminate, readily soluble and readily washable sodium sulfate and insoluble alumina are formed as reaction products.
The alkali silicate or sodium aluminate is added in an amount to obtain a pH value of 4 to 9, preferably 7 to 8. The temperature is in the range of 25 ℃ to 80 ℃, preferably in the range of 25 ℃ to 60 ℃.
In one embodiment of the invention, the neutralization is carried out by hydrothermal method (hydrotherm method) under conditions of elevated pressure and temperature.
Subsequently, the neutralized titanium dioxide is filtered, washed and heat-treated. The heat treatment is carried out in agglomerates known to the person skilled in the art, for example in a spray dryer, a conveyor dryer or a rack dryer. The temperature is about 100 ℃ to 140 ℃. A nanoparticulate crystalline titanium dioxide product having the anatase structure is obtained. Alternatively, the neutralized, filtered and washed titanium dioxide may be pelletized and dried by an extruder, optionally with an additional binder.
The dried product has an agglomerated structure and contains nanoparticulate titanium dioxide and neutralized silica and/or alumina product. Depending on the drying process, the agglomerate size is at least about 500 μm, preferably 500 μm to several mm, more preferably 500 μm to 10mm, most preferably 500 μm to 5 mm. A specific surface area according to BET of about 200 to 400m2A/g, preferably from 200 to 300m2(ii) in terms of/g. The dried agglomerates can be dispersed in water or solvent in the usual manner, wherein the agglomerate size will be reduced to 1 to 5 μm.
The nanoparticulate titanium dioxide product according to the invention is characterized by a high adsorption capacity for heavy metals and polar compounds. It is suitable as a photocatalyst, process catalyst or adsorbent and is preferably used in the field of gas purification, in particular in the field of purification of aqueous systems.
The nanoparticulate titanium dioxide obtainable by the process disclosed herein forms a further part of the invention.
The invention also includes the use of the nanoparticulate titanium dioxide obtainable by the process described herein as an adsorbent, a photocatalyst or a process catalyst.

Claims (14)

1. A process for preparing nanoparticulate titanium dioxide comprising the steps of:
(i) providing an aqueous solution of an acidic titanyl compound;
(ii) hydrolyzing the titanyl compound to produce a titanium oxide-hydrate suspension;
(iii) filtering the suspension and washing the resulting titanium oxide-hydrate filter cake;
(iv) neutralizing the filter cake; and
(v) heat treating the filter cake;
characterized in that the neutralization is effected by adding an aqueous solution of an alkali aluminate or by adding aqueous solutions of an alkali silicate and an alkali aluminate.
2. The method of claim 1, wherein the aqueous solution of alkali aluminate has an alkali aluminate concentration of 2 to 20 mole percent, and the aqueous solution of alkali silicate and alkali aluminate has an alkali silicate concentration of 2 to 20 mole percent and an alkali aluminate concentration of 2 to 20 mole percent.
3. The method according to claim 1 or 2, characterized in that the pH is adjusted to 4 to 9 during the neutralization.
4. The method according to claim 3, characterized in that the pH is adjusted to 7 to 8 during the neutralization.
5. The method according to claim 1 or 2, wherein the acidic titanyl compound is titanyl sulfate.
6. The method of claim 5, wherein the titanyl sulfate is obtained during the sulfate process for producing titanium dioxide.
7. A method according to claim 1 or 2, characterized in that the nanoparticulate titanium dioxide in agglomerated form has an agglomerate size of at least 500 μ η ι.
8. The method of claim 7, wherein the nanoparticulate titanium dioxide in agglomerated form has an agglomerate size of 500 μ ι η to 10 mm.
9. The method according to claim 1 or 2, characterized in that the nanoparticulate titanium dioxide in agglomerated form has 200 to 400m2Table of ratios according to BET/gArea.
10. The method of claim 1, wherein the nanoparticulate titania is dispersed in a solvent.
11. The method of claim 1, wherein the nanoparticulate titania is dispersed in water.
12. The method of claim 10 or 11, wherein the dispersed nanoparticulate titania has an agglomerate size of 1 to 5 μ ι η.
13. Nanoparticulate titanium dioxide obtained by the process according to any one of claims 1 to 12.
14. Use of the nanoparticulate titanium dioxide according to claim 13 as an adsorbent, a photocatalyst or a process catalyst.
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